Purification of highly-oxidizable metals



R. W. MOORE PURIFICATION OF HIGHLY OXIDIZABLE METALS `lan. 5 1926.

Filed March 2 1923 2 Sheets-Sheet l v ..6 .n P/ t o u wm. A Wm mw Rf V. .D

R. W. MOORE PURIFICATION OF HIGHLY OXIDIZABLE METALS Jan. 5 1926.,

Filed March 2 1923 2 Sheets-Sheet 2 Irm/entor Roy W. Moore,

HIS Attorney.

30 less fusible non-metallic constituents.

Y W. MOORE, F SCEENECTADY, NEW YORK, ASSIGNOR T0 GENERAL ELECTRIC' v COMPANY, A CORPORATION 0F NEW YORK.

PURIQEICATION OF HIGHLY-OXIDIZABLE METALS.

application led March 2, 1923. Serial No. 622,240.

To all whom t may 'concer/n.'

Be itlmown that I, ROY MOORE, a citizen of the United States, residing at Schenectady, in the county of Schenectady, State of New York, have invented certain new and useful Improvements in Purification of Highly-OXidizable Metals, of which the following is a specification.

The present invention relates to the prepalo ration of homogeneous, coherent masses of highly oxidizable metal, such as uraniumwhich heretofore has been obtained only in an impure, granular state. Y 0

As a consequence of my invention metallic 16 uranium is rendered available in a coherent and ductile state.

Heretofore, metallic uranium has been available either as very small pellets which developed cranks when mechanically de- 20 formed or as rods of sintered, or loosely coanhydrous chloride of uranium with an alkali metal, is heated somewhat above the fusing temperature of uranium under inert conditions and the substantially pure metal is withdrawn in a fused condition from the ile novel features of my invention will be pointed out in detail in the appended claims.

The accompanying drawing shows in Fig. 1 a vertical section of an apparatus suitable for reducing uranium from its compounds and Fig. 2 shows in'vertical section one form of a puriication'apparatus.

In carrying out my invention, I prefer to utilize for reduction the dense, substan- 40 tially anhydrous chloride, UCL, which is formed by the interaction of uranium oxide and sulphur monochloride. Thischloride of uranium preferably is purified by sublimation and preferably protected from the atmospherc by dry nitrogen until it is used for reduction. As a reduction agent, I prefer to use resublimed, purified sodium. About y 25% in excess of the amounty of sodiumv theoretically necessary preferably is used.

The reaction between the uranium chloride and sodium is ,carried out in a con-4 .55; with a threaded 'cap 2. .This container or bomb under the protection of dry nitrogen,`

the plug 2 is screwed in place with an interposed gasket but the joint is not made erfectly gas-tight. The bomb is place in good thermal relation with an electric heater 6 wound on an alundum tube 7 or other suitable support. A shield 8 consisting of an alundum tube surrounded by a metal shell may be provided outside of the heater 6. Current is conveyed to the heater b the sealed-in condu tors 9, 10. The cham er 3 and the bomb 1 may be .exhausted simultaneously by a tube 11. After exhausting to about 25 microns, heat is applied by the electric heater 6 untilA the reaction occurs with a sudden rise of temperature. The temperature may be observed by any suitable means such as a thermocouple l2. After` cooling, the vacuum is broken by admitting nitrogen to the receptacle 3.

. The reduction product is a sintered grayish mass comprising uranium, sodium, sodip-um chloride, unreduced luranium. chloride and impurities. It is washed successively dilute acetic acid, water and acetone.

heavy, brownish powder containing I pellets about one to 'two millimeters in i diameter remains which consists largely of `metallic uranium together with some uranium oxide.

This material unlike tantalum cannot be purified by the volatilization of impurities 'from the impurities in an inert environment and under such conditions that no alloyage occurs.

With this end in view the fusion is carried out in an apparatus such as shown in Fig. 2, by an arc in the resence of a r1gas of the helium group, suc as' argon. his apparatus comprises a container 15, consisting of transparent material such as glass or quartz, rovided `with water-cooled electrodes and 16, l ,passing through rubber Stoppers 18,

19. The u per electrode 16 assumes the oxide when exposed toair for a few days'.

ormgo a c amp for holding a disc 20 of The metal is ductile and permits mechanical uranium and the lower electrode provides Vworking cold. Ingots have been converted a depression 21 for collecting fused uranium. into the form of thin sheets by rolling cold. 40

The gaseous contents of the container may What 'I claim as new and desire to secure be exhausted and a selectedv as may be by Letters Patent of the United States, isf-- admitted by a tube 22. The isc 20 may 1. The process of separating uranium consist of the impure 4reduction product from. a less fusible oxide which consists in pressed into coherent form in a suitable usin said metal under inert conditions and mold, and sintered by an are in a rare gas wlth rawing the fused metal from the less to improve the strength., .fusible oxygenous material.

A similarv loosely coherent disc or discs The process of treatin non-ductile 23 of uranium are placed on the-ed e of the uranium containing compoun s of uranium lower electrode 17 which refera ly con- .which consists in fusing said metal in an sistsV of `iron or Monel meta and is so thin atmosphere of'a as of the helium group and lfused metal from the less as to be maintained lby the cooling water at separating the a tem erature too lowto permit alloyage fusible impurities.

with the melted uranium. -.N 3. The process of treating granular, im-

Ater the container has beensexhausted pure uranium which consists in heating said and washed with argon, a direct'current arc material in argon gas tothe fusing temo about 200 amperes is started between the perature of uranium, mechanically separatelectrodes in argon gas at about 75'to100 mg'fused metal from less fusible impur-i microns. For example, the electrode 16 is ties and collecting the fused metal as a subushed downwardly until the disc, 20 comesf-stantially homogeneous mass. into contact with disc'or dlscs 23, the upper 4.L .The rocess. of converting impure electrode then being withdrawn to strike an inely divi ed uranium to a coherent state arc. By manipulation of the arc and by which consists in heating said metal in an tilting the apparatus, the fused uranium inert environment to a temperature suican be caused to run into the depression 2l ciently high to fuse uranium while leaving and collected in a substantially pure state. impurities therein intact and causing the If the electrode 17 is kept vwell. cooled no fused metal tofiow away from unfused imallo age takes place. f puritiese uranium pig metal 'thus formed has In witness whereof, I have hereunto set the appearance of olished iron. The metal my hand this 28th day of February, 1923. oxidizes readily, arightly polished surface of urani becomes tarnished with brown BUY W. MOORE. 

